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目的:建立以固相萃取-高效液相色谱法测定西罗莫司血药浓度的方法。方法:采用Waters OASIS固相萃取柱处理血样后进样分析,其中色谱柱为Supelcosil LC-18DB,流动相为甲醇-水(75∶25),流速1.5mL·min-1,检测波长276nm,柱温50℃。结果:西罗莫司血药浓度在1.25~70ng·mL-1范围内与峰面积比线性关系良好(r=0.999 7),最低检测浓度为0.5ng·mL-1;平均方法回收率为(101.7±2.7)%,萃取回收率≥82.8%,日内RSD≤4.0%,日间RSD≤5.4%。结论:本方法简便快速、灵敏准确,可用于西罗莫司血药浓度的快速监测。
Objective: To establish a method for the determination of plasma concentration of sirolimus by solid phase extraction - high performance liquid chromatography. Methods: The sample was analyzed by Waters OASIS SPE column. The chromatographic column was Supelcosil LC-18DB. The mobile phase was methanol-water (75:25), the flow rate was 1.5 mL · min-1, the detection wavelength was 276 nm. Temperature 50 ℃. Results: There was a good linear relationship between the concentration of sirolimus and peak area in the range of 1.25 ~ 70 ng · mL-1 (r = 0.999 7) and the lowest detection concentration was 0.5 ng · mL-1. The average recoveries were 101.7 ± 2.7)%, the recovery rate of extraction was more than or equal to 82.8%, the RSD≤4.0% and the daytime RSD≤5.4%. Conclusion: The method is rapid, sensitive and accurate and can be used for the rapid monitoring of plasma concentration of sirolimus.